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The effects of chemical composition and preparation conditions, especially calcination atmosphere on the catalytic performances of silica-supported MoVTeO catalysts for the selective oxidation of propane to acrolein have been studied. Among the catalysts studied, the MoV0.2Te0.1/SiO2 catalyst calcined in inert atmosphere showed the best performance in terms of propane conversion and selectivity to acrolein. The results of XRD, XPS and Raman revealed that the calcination atmosphere affected greatly the catalysts in many ways including structure, chemical composition and Mo oxidation state, which are related to their catalytic performances. (c) 2006 Elsevier B.V. All rights reserved.